反应 #1202900
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04057418
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1 g of concentrated sulfuric acid was added to 2.32 g (10mmoles) of 2,5-dichloro-3-aminobenzoic acid ethyl ester, 2.27 g (11mmoles) of hydroxymethyl-(4-chlorophenyl)-sulfone and 40 ml of water whilst stirring at room temperature. The mixture was stirred for a further 3 hours at room temperature, the solid was filtered off and dissolved in about 100 ml of methylene chloride, the solution was dried over magnesium sulfate and worked up in the usual manner and the product was recrystallized from ethylene chloride. 3.0 g (71% of theory) of 2,5-dichloro-3-[(4-chlorophenyl)-sulfonylmethylamino]-benzoic acid ethyl ester were obtained in the form of colorless crystals of melting point 173°-175° C. The mixture was stirred for a further 3 hours at room temperature the solid was filtered off dissolved in about 100 ml of methylene chloride the solution was dried over magnesium sulfate the product was recrystallized from ethylene chloride
来源 ID: ord-940a81a65d644590b07f98b76862b519